Method of making fluorids and silicates.



t ll {till X UNITED STATES WALTER MILLS, OF Loxnox. ENGLAND, AssIoxoa To a. o.- GRANGER,

or CARTERSVILLE, ononom. i

METHOD OF MAKING FLUORIDS AND SILICATESYL,

Patented March 22, 1904 PATENT ()F IGE.

SPECIFICATION forming part of Letters Patent No. 755,379, dated March 22, 1904. Application filed May 25, 1903. I Renewed February 24,1904. Serial No. 195,111. (No specimens.)

To all whom it may concern:

Be it known that I, WALTER MILLS, asubject of the King of Great Britain. residing in London, England, have invented certain new and useful Improvements in Manufactures of Fluorids and Silicates, of which the following is a specification.

This invention relates to the manufacture of fluorids and silicates of various metals, whose silicofluorids are obtained from silicofluorid of lead prepared readily and economically by the reaction between metallic lead or its ores and hydrofluosilicic acid, which when sufiiciently concentrated, and particularly when the concentrated acid is heated, readily attacks and dissolves metallic lead and its ores, especially galena and cerusite.

In carrying the present improvements into practice a solution of silicofluorid of lead is prepared by acting upon excess of'lcad'or'of the crushed ores with hydrofluosilicic acid, the mixture being placed in a pan or other proper receptacle and heat being applied until the mass is substantially dry. I tin'd that the acid begins to attack and dissolve thesubstance when its specific gravity is about 1.80 In the event that scrap-lead is used the action of the acid is somewhat accelerated by blowing air. through the mass. 'arm water is then added to the substance in the pan, whereby an aqueous solution of silicofluorid of lead is obtained. By adding to this aqueous solution nitrate of calcium, potassium, or sodium, either in aqueous solution or in" tine powder, the silicofluorid of the respective metals is precipitated, while nitrate of lead remains in solution. After drawing off the. nitrate of lead the silicofluorid is first washed and then dried atabout 100 centigrade and the temperature then gradually raised. At about 350 centigrade the silicolluorid is decomposed into a metallic fluorid and gaseous silicon tetrafluorid. This gas may be brought into contact with water by any convenient means, whereupon the well-known don ble re action takes place, hydrofluosilicic and silicic acids being produced in accordance with the equation A small quantity of the silica dissolves in the hydrofluosilicic acid, but almost all is precipitated 'hen washed with water and dried, almost chemically-pure silica in an exceedingly fine state of division is thus obtained.

For the purpose of manufacturing the respective silicatesas, f u-'instancc, the silicate of sodium or potassium-4 mix finely-divided sand or similar silicions material with the metallic silicofluorid in approximately molecular proportions and then beat the mixture to a slightly-greater extent than when preparing the metallic iluorids, as aforesaid. Under these circumstances all the fiuorin is expelled from the mixture, which when, sodium silicofiuorid is used undergoes a reaction in accordance with the equation 2XHQSlFB+sslOa sxtla los'iaslFt.

The silicon tetratluorid may be used as before for the preparation of hydrotiuosilicic acid.

It is to be understood that I do not confine myself to the preparation of silicates of sodium and potassium containing silica in precisely the proportions indicated by the equation. \Yhere silicates containing a greater proportion of silica are required, I obtain them by increasing the quantity of silicious material which is mixed with the metallic silicotluorid.

Having described my invention, I claim- 1. The process of manufacturing metallic fluorids which consists in precipitating'the silicofiuorid of the metal from a solution of 'silicofluorid of lead by adding thereto a nitrate and then subjecting the precipitated silicotluorrd to the requisite amount of heat to form the compound desired.

:2. The process of manufacturing metallic fluorids which consists in precipitating the silicotiuorid ot' the metal from a solution of SlllC0llllOl'l(l of lead by adding thereto an alk-a-li nitrate, and then s'ubjecting'the precipita'ted siiicuflnorid to the-requisite ameunt of heat to -f01 m the compound desired.

3. The process of; manufacturing metallic -5' fiuorids which emsists in. dissolving leadcarrying. substancesin heated concentrated hydrofluo siiieic acid in then precibitating the hydrdflnosilicic' aid with an; alkali-nitrate; and'in then subjecting the precipitated silicomfluorid 'to' the requisite amount of heat to form the-compound desire-d.

' 4:. The prpcessf manufaeturing'metallic silicates which cens'ists in dis solving leadjor a moop a lead -'carrying compound in heated concentrated hydroflnosilicic acid; in then precipitating the hydrofludsilicic acid with-e nitrate; in then mixing thept'eeipi'tated. -silicofiuorid. witlfsilicious, in'ateriai; and'in then-subjecting the mixture to the requisite amount ofheat toform'the, silicate desired.-

Signed at Nos. 9 to 15 Murray street, .New York, N. Y., this 23d day of May, 1903.

WALTER MILLS.

Witnesses:

FRED. J. DOLE, JOHN O. SEIFEBT: 

